Triethylamine → HCID 16039366, Verbindung

HRID 639284Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 639284
[Cl:1][C:2]1[CH:28]=[CH:27][C:5]([O:6][CH2:7][C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[C:21]([C:24](Cl)=[O:25])=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1.C(N(CC)CC)C.Cl.[CH3:37][C:38]1[C:43]([NH2:44])=[CH:42][CH:41]=[C:40]([C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][C:46]=2[CH3:51])[CH:39]=1>O1CCCC1>[Cl:1][C:2]1[CH:28]=[CH:27][C:5]([O:6][CH2:7][C:8]([N:10]2[C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=3[CH2:14][N:13]3[C:21]([C:24]([NH:44][C:43]4[CH:42]=[CH:41][C:40]([C:45]5[CH:50]=[CH:49][CH:48]=[CH:47][C:46]=5[CH3:51])=[CH:39][C:38]=4[CH3:37])=[O:25])=[CH:22][CH:23]=[C:12]3[CH2:11]2)=[O:9])=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 1488202',3-Dimethyl-4-aminobiphenyl hydrochlorideHCID 86607493HCID 86607493, Verbindung

Produkt 1

HCID 16039366HCID 16039366, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a stirred solution of 10-[2-(4-chloro-phenoxy)-acetyl]-10,11-dihydro-5H-benzo[e]pyrrolo[1,2-a][1,4]diazepine-3-carbonyl chloride of step B (0.415 mmol) in anhydrous tetrahydrofuran (3 mL) was added triethylamine (0.829 mmol) and 3,2′-dimethylbiphen-4-ylamine hydrochloride (0.415 mmol). The solution was stirred for 18 hours at ambient temperature. The solvent was evaporated, the residue was taken up in dichloromethane, washed with water, dried over anhydrous sodium sulfate, and evaporated. Chromatography on silica gel using 55:23:22 hexane/ethyl acetate/dichloromethane as eluant gave the title compound as an amorphous solid. This was crystallized from ethyl acetate/hexane to afford 0.17 g of the title product (71% yield), m.p. 159-161° C. MS [(+)ESI, m/z]: 576 [M+H]+ Anal. Calcd for C35H30CIN3O3: C, 72.97; H, 5.25; N, 7.29. Found: C, 72.59; H, 5.28; N, 7.24.

Aufarbeitung

  1. customThe solvent was evaporated
  2. washwashed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-a2536bb5ca904b5db659b6dc7f971f0f
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07691848B2

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